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Flow Enhanced Electrochemical Sensor Performance in Complex Salt Systems

To advance MSR MC&A practices, Argonne National Laboratory developed and optimized robust flow enhanced electrochemical sensors (FEES) and multielectrode array voltammetry sensors (MAVS) which provide accurate near-real time measurements of actinides in molten salts. Flow-enhanced electrochemical sensors are installed directly into MSR flow conduits for inline salt chemistry measurement, while MAVS are deployed in quiescent salt conditions enabling online species concentration determination in stationary salt vessels. This report summarizes efforts to improve electrochemical sensor technological readiness through (1) sensor testing in complex, high concentration molten salt systems to demonstrate low uncertainty actinide measurements in MSR-representative solutions and (2) demonstrations of sensor performance in challenging real-world conditions in collaboration with partner MSR institutions.

22 GENERAL STUDIES OF NUCLEAR REACTORS

Thermochemical measurements of FeCl 2 in LiCl via electromotive force, coulometric titration, and cyclic voltammetry

The thermochemical properties of FeCl 2 in the LiCl-FeCl 2 binary system were determined at 913 K using electromotive force (emf) cells containing pre-made and coulometrically titrated molten salt compositions. Coulometric titration to in-situ change the salt composition utilizes the multiple valences of Fe ions and the tendency of Fe 3+ ions to comproportionate with Fe metal, forming additional Fe 2+ . The emf results were used to define the compositions in which Henry’s law is applicable, up to approximately 2 mol% FeCl 2 . Thermochemical quantities were determined from emf using a Standard Lithium Chloride Electrode (SLiCE) which defines 0 V as the reduction of Li + in pure LiCl at all temperatures. Validation of emf measurements was performed by comparing the formal potential measured by using cyclic voltammetry (2.224 ± 0.013 V vs SLiCE) and emf measurements (2.236 ± 0.004 V). In conclusion, this work shows that coulometric titration of an electroactive species that undergoes comproportionation can be used to rapidly obtain granular emf data in molten salt systems.

Coulometric titration

SULI Report - Development of a Molten Salt Circulation Loop for in-situ Spectroscopy

This project supports the development of real time optical monitoring capabilities for molten salt reactor (MSR) environments by designing, testing, and refining a molten salt circulation loop suitable for combined laser induced breakdown spectroscopy (LIBS) and ultraviolet visible (UV Vis) absorption measurements. Online spectroscopic monitoring is increasingly important for nuclear safeguards, corrosion tracking, and material accountancy, yet MSR process fluids present substantial challenges due to their chemical complexity and hazards such as high temperatures and radiation. To address these needs, this work focuses on Phase I, the development of a room temperature aqueous circulation loop that serves as a surrogate platform for evaluating flow behavior, optical access, and component performance prior to high temperature salt operation. Initial testing identified several practical issues—including leaks, obstructions, and two-phase flow through the absorption cell—that were systematically resolved through hardware replacement, flow path redesign, and venturi pressure optimization. Relocating the flow cell upstream of the primary venturi enabled periods of stable single-phase flow, demonstrating the feasibility of integrating optical diagnostics into a circulation system. The results of Phase I provide essential design insight for Phase II, which will incorporate furnace compatible materials and LiCl KCl eutectic salt. Completion of the molten salt system will deliver a reusable testbed for evaluating multimodal spectroscopic techniques, advancing nondestructive, real time monitoring tools for future MSR and nuclear fuel cycle applications.

98 - NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL

Dry Deactivation of Sodium Metal in a Molten LiCl-KCl-CsCl-NaCl System

An experimental study was performed with the objective of investigating and characterizing a dry technique for deactivation of sodium metal in a molten salt system. The study was performed in three parts. First, proof-of-principle testing of the technique was performed at bench scale. It involved loading and melting tens of grams of clean sodium metal atop a pool of LiCl-KCl-CsCl eutectic at ∼300°C and then adding ammonium chloride particles while mixing. The ammonium chloride reacted with sodium to form sodium chloride and nitrogen/hydrogen off-gases. The sodium chloride assimilated into the salt pool, forming a quaternary salt mixture of LiCl-KCl-CsCl-NaCl. The proof-of-principle testing repeatedly exhibited complete deactivation of the loaded sodium metal. Second, characterization of a LiCl-KCl-CsCl-NaCl system was performed using differential scanning calorimetry to produce a partial phase diagram of LiCl-KCl-CsCl eutectic versus NaCl, which identified the liquidus, solidus, and two-phase regions of the quaternary system. Third, the dry deactivation technique was demonstrated at kg-scale in an inert atmosphere radiological glovebox with sodium metal that was previously separated in the same glovebox from uranium metal in unirradiated blanket elements for the Fermi-1 nuclear reactor. The quaternary salt product at the end of the demonstration was sampled and showed complete deactivation of the sodium metal. Here, in short, this study qualified a technique to completely deactivate batches of sodium metal in the absence of air or water. While this study focused on the deactivation of sodium metal, including bond sodium from unirradiated blanket elements, the technique is applicable to other sources of sodium metal, such as sodium metal from batteries. Furthermore, the technique could also be extended to other alkali metal systems, including lithium, sodium, potassium, rubidium, cesium, and mixtures thereof.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Molten Halide Salt Surface Tension: Methods and Correlations

Here, this paper reviews various methods for studying surface tension and their applicability to fluoride and chloride molten salt systems, including a comparison of benefits and drawbacks. Such a comparison aids in experiment design based on desired factors such as scale, accuracy, and repeatability. A detailed review is presented for existing literature data regarding the surface tension of molten fluoride and chloride salts. These reference data were compiled and analyzed to determine cross-validated correlation equations for several alkali and alkaline earth fluoride and chloride salts as functions of temperature. These correlations are necessary for reliable multiphysics modeling approaches as well as accurate design and analysis of multiphase molten salt phenomena such as gas sparging and bubble formation/transport. This analysis supports the development of the thermophysical arm of the Molten Salt Thermal Properties Database (MSTDB-TP) managed by Oak Ridge National Laboratory.

Chloride

The Radiation-Induced Fate of Fission Product Iodine in Molten Salts

Understand and Predict Radiation-Induced Iodine Speciation, Chemistry, and Transport in High-Temperature Molten Salts Award Number: DE-AC07-05ID1451 Gregory P. Holmbeck (Gregory.Holmbeck@inl.gov), Center for Radiation Chemistry Research, Idaho National Laboratory, 1955 N. Fremont Avenue Idaho Falls, ID, 83415, USA. Project Scope The goal of this Chemical and Materials Sciences to Advance Clean Energy Technologies and Low-Carbon Manufacturing project is to understand and predict the radiation-induced speciation, chemistry, and transport of fission product iodine in the triumvirate extremes of high-temperature, ionizing radiation, and corrosive molten salts. This missing fundamental information is critical for the accelerated development and deployment of safe, clean nuclear energy based on molten salt reactor (MSR) and pyrochemical reprocessing technologies. The central hypothesis driving this research is, the radiation-induced conversion of iodide will yield an extensive suite of transient and steady-state iodine radiolysis products that will alter the bulk chemical and physical properties of the irradiated molten salt system—the speciation, distribution, and chemical transport of which will be dictated by the composition and the availability of multivalent metal cations and metal alloy interfaces. To test this hypothesis, this project initiated three synergistic Research Objectives: (1) determine how the inclusion of iodine/iodide influences the chemical and physical properties of complex molten salt mixtures; (2) elucidate the speciation and fundamental chemical behavior of transient and steady-state iodine/iodide species formed by the irradiation of molten and solid salt mixtures; and (3) understand the influence of interfacial processes on determining the final disposition of iodine in high temperature molten salts, notably the structure and chemical speciation of iodine at metal-salt interfaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Design, Construction, and Installation of In-Glovebox Pumped Actinide Molten Salt Loops

This report summarizes the work conducted in FY25 to construct and install pumped actinide-bearing molten salt loopsin a radiological glovebox. The establishment of such a capability will provide a platform in which technologies developed for Gen. IV molten salt reactors may be tested under relevant operating conditions. A review of convective molten salt systems is provided to frame Argonne’s pumped actinide loop relative to contemporary and historical systems. Moreover, the infrastructure needed to operate the system is detailed to provide additional context as to design metrics of the loops and supporting equipment. The pumps’ performance in water testing is outlined and used to inform operational activities planned in FY26. Finally, electrochemical experiments investigating fundamental reaction mechanisms governing reactive oxygen species that promote corrosion of molten salt media is also reported. In total, these combined loop installation and sensor development tasks will serve to aid in the future commercial deployment of molten salt reactors in the U.S.

22 GENERAL STUDIES OF NUCLEAR REACTORS

Design Status and Experimental Strategy for Initial Molten Salt Irradiation Experiments in HFIR

The development and deployment of molten salt reactor (MSR) technologies require experimental capabilities that can evaluate molten fuel salt behavior and structural material performance under representative irradiation conditions. Although modeling and separate effects testing provide important insight, there remains a critical lack of in-pile data that capture the coupled effects of neutron irradiation, temperature, salt chemistry, and time. Informed by lessons learned from historical MSR programs and recent international irradiation efforts, this report presents a structured approach to addressing existing gaps in molten salt irradiation testing using the High Flux Isotope Reactor (HFIR). A phased irradiation strategy is presented that incrementally increases experimental complexity while managing cost, risk, and facility constraints. The framework progresses from passive, nonfueled static capsule experiments to fueled, instrumented, and ultimately circulating molten salt systems, providing a pathway for materials screening, mechanistic understanding, and qualification-relevant testing. The report defines a near-term Phase 1 passive capsule concept, associated irradiation conditions, and a conceptual post-irradiation examination strategy. Ongoing modeling, out-of-pile testing, and safety analysis activities are described to support continued capability maturation and to enable future phases of molten salt irradiation testing in support of MSR technology deployment.

22 GENERAL STUDIES OF NUCLEAR REACTORS

Computational Fluid Dynamics Analysis of the Molten Salt Tritium Transport Experiment Test Section

Tritium, a radionuclide produced through neutron capture by lithium and other elements (beryllium and fluoride) in molten salts, presents unique challenges to radionuclide release. This is true for both fusion energy breeder blankets and molten salt fission reactors. The fundamental understanding of tritium transport is crucial to the safe design and operation of these reactors. The Molten Salt Tritium Transport Experiment (MSTTE), currently under construction at Idaho National Laboratory, aims to investigate tritium transport phenomena using a forced-convection fluoride salt loop. This loop is designed to study various transport mechanisms, such as permeation through metals and gas-liquid interactions, and is intended to support future research on tritium extraction units. A critical aspect of the MSTTE loop design is ensuring a fully developed velocity profile before the fluid reaches the permeation test section where measurements are made. This study employs computational fluid dynamics to model the salt flow behavior within the MSTTE permeation test section. A realizable k-ε turbulent model with enhanced wall treatment is used to simulate the single-phase, vertical upward flow of molten salt FLiNaK under isothermal conditions. The simulation results indicated flow distortion and underdeveloped profiles at all planned flow rates within the test section due to the 85-deg sharp bend. To address this issue, a reduced diameter with a reducer and expander and a flow conditioner are investigated to achieve fully developed flow. The analysis showed that the flow conditioner successfully corrected the flow profile, achieving fully developed behavior at a flow rate of 50 liters per minute (LPM). In conclusion, this research enhances our understanding of flow dynamics in molten salt systems and contributes to optimizing tritium transport control technologies.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Computing chemical potentials with machine-learning-accelerated simulations to accurately predict thermodynamic properties of molten salts

The successful design and deployment of next-generation nuclear technologies heavily rely on thermodynamic data for relevant molten salt systems. However, the lack of accurate force fields and efficient methods has limited the quality of thermodynamic predictions from atomistic simulations. Here we propose an efficient free energy framework for computing chemical potentials, which is the central free energy quantity behind many thermodynamic properties. We accelerate our simulations without sacrificing accuracy by using machine learning interatomic potentials trained on density functional theory (DFT) data. Using lithium chloride as our model system, we compute chemical potentials with DFT-accuracy for solid and liquid phases by transmuting ions into noninteracting particles. Notably, in the liquid phase, we demonstrate consistency whether we transmute one ion pair or the entire system into ideal gas particles. By locating the temperature where the chemical potential of solid and liquid phases cross, we predict a melting point of 880 ± 18 K for lithium chloride, which is remarkably close to the experimental value of 883 K. With this successful demonstration, we lay the foundation for high-throughput thermodynamic predictions of many properties that can be derived from the chemical potentials of the minority and majority components in molten salts.

Gibson, Luke D. [Oak Ridge National Laboratory (OR

Corrosion of Wrought and LPBF 316H in Molten Eutectic Na-Mg Chloride Salt

This presentation shows experimental work at INL evaluating the corrosion behavior of wrought and laser powder bed fusion (LPBF) 316H stainless steel (SS) in chloride molten salt systems. This evaluation focuses on understanding the relationship between the material’s as-built characteristics and its corrosion performance, the effects of acid cleaning and descaling before corrosion.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Root cause analysis of a molten salt pump in FLUSTFA

The primary salt pump installed in the high-temperature FLUoride Salt Test Facility (FLUSTFA) was successfully operated for some time, but later ceased operation. To understand what occurred, a Root Cause Analysis (RCA) was performed. Steps taken to try to get the pump operational include adjusting the shaft position, increasing the heating power of the tape heaters on the pump volute, and manually rotating the pump shaft. While removing the insulation, corrosion was noted on the outside of the pump volute, and decolorization of the insulation and tape heaters was observed. Significant corrosion products were also observed in the pump itself and the piping connected to the pump. The nitrogen cover gas was maintained from before salt was introduced into the loop until the pump was dismounted and continues to be maintained even after the pump was removed. After considering probable scenarios, causes were assigned and corrective actions were developed to prevent those causes. Then, the RCA was presented to an advisory committee for review, the “Review Committee,” consisting of experts in large molten salt systems: Brandon Haugh, David Holcomb, Kevin Robb, and Vicente Rojas. As a result, the advisory committee provided comprehensive feedback, which have been incorporated into a revised RCA. Findings have then been summarized and reported in this publication.

22 - GENERAL STUDIES OF NUCLEAR REACTORS

Real-time monitoring of trace noble gases using laser-induced breakdown spectroscopy—An investigation of the impact of bulk gas on plasma properties and sensitivity

The impact of Ar and He bulk gases on laser-induced breakdown spectroscopy (LIBS) real-time monitoring of trace Xe and Kr was assessed. LIBS is being developed as a monitoring tool for measuring noble gas transport in molten salt systems, in which traditional sensors may face challenges associated with radiation, corrosive materials, and/or mixed phases. The plasma temperature and electron densities of LIBS plasmas were measured in both static and various flowing Ar and He streams (0–5 L min −1 ). The use of an Ar bulk gas resulted in higher plasma temperature, greater electron densities by an order of magnitude, and extended plasma lifetime compared with when He bulk gas was used. Gas flow rate was found to have little impact on plasma temperature; however, its effect on electron density was significant, indicating the need to consider flow rate–specific models. Matrix effects on emission peaks were reported for both bulk gases. Due to these matrix effects, multivariate models were developed for Xe and Kr ranging from 0 to 700 ppm in both bulk gases. Although the predictive behavior was similar (root mean square error of prediction ranging from 11.1 to 20.6 ppm), the limits of detection were superior in He (Xe: 22.9 ppm, Kr: 30.4 ppm). Furthermore, these models were employed in demonstrative real-time tests (>1 h), which showed strong predictive precision (relative standard deviation <5 %) regardless of the bulk gas. Ultimately, this study provides a guide for the considerations required when developing gaseous LIBS models for real-time monitoring.

Gas flow effects

Multiphase Species Transport Modeling for Molten Salt Reactors in the System Analysis Module: Generation, Decay, Deposition, and Extraction of Insoluble Fission Products

With the increase of interests in the design and deployment of advanced reactor systems, a desire for simulation tools supporting system analysis of reactor operation and safety is rising. Molten salt reactors (MSRs), one of the advanced reactor systems, utilize liquid fused salt fuel as both coolant and fuel. During operation, MSR generates insoluble fission products, including noble metals and gases. The buildup of these species in fuel salt presents safety concerns as they may deposit on surfaces of critical components and produce excessive decay heat, causing the failure of system components. Timely removal of these noble metals and gases would ensure the safe operation of the reactor system. The dynamic nature of salt fuel system, involving the generation, decay, deposition, and extraction of noble metals and gases, calls for robust species transport models to facilitate system analysis and monitoring, and design of efficient species removal components. This paper concentrates on the development of a computational framework for species transport, consisting of multiphase transport model formulation, mass transfer between phases, numerical implementation in MOOSE environment, verification through Method of Manufacture Solutions (MMS) and validation against experimental data from the Molten Salt Reactor Experiment (MSRE). Integrating this framework into the System Analysis Module (SAM) code further enhances SAM’s capabilities for advanced reactor analysis in the future.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS

MSTL Re-Start Phase 1.5 Project Final Report

This document provides an overview of re-start efforts at Sandia National Laboratories (SNL), National Solar Thermal Test Facility (NSTTF), for the SNL Molten Salt Test Loop (MSTL). MSTL is one of the world’s only industrial-scale molten salt test systems, capable of testing commercial-scale thermal hydraulic equipment at an industrial scale, required for confident bankability of products. This work was facilitated as part of the Phase 1 re-start effort for facilitating forensics assessments to inform final refurbishments and upgrades costs and schedule information for revitalizing MSTL for use during a separate Phase 2 effort. This work was facilitated to further de-risk a Phase 2 effort pertaining to the tank and the pump, which were considered during Phase 1 to be high-risk items for a successful re-start. Impact from a successful re-start will allow SNL and other industrial molten salt systems companies, such as those in the Market Utilization Report provided in the Phase 1 submission package. An objective of this document is to also ensure longevity of utilization of MSTL after re start.

14 SOLAR ENERGY

Application of a Triple Bubbler Inside Molten Salt for Pyroprocessing Safeguards Purposes

The application of a triple bubbler system within molten salt environments, specifically a eutectic mixture of LiCl-KCl, is explored for nuclear safeguards purposes, focusing on nuclear material accountancy (NMA) and holdup accountancy in pyroprocessing techniques. Traditional holdup accountancy methods, which involve periodic sampling and lengthy lead times, are being supplemented by the development of actinide sensors using electrochemistry. However, these methods alone are insufficient to meet regulatory requirements set by agencies like NRC and IAEA. The triple bubbler device measures salt level, density, and surface tension simultaneously using three dip tubes of varying diameters and heights. This study investigates the accuracy and robustness of the triple bubbler in molten salt conditions at temperatures ranging from 450-550°C. The updated bubbler design, utilizing tantalum metal and larger tube geometry, demonstrated minimal plugging and maintained measurement accuracy within acceptable uncertainties: 0.611% for depth, 1.34% for density, and approximately 40% for surface tension. Results indicate that the triple bubbler system is effective for real-time, accurate measurements in pyroprocessing environments, making it a promising tool for ensuring compliance with nuclear safeguards and supporting nuclear non-proliferation efforts.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS